CN105460899B - A kind of preparation method of the exfoliated layered double-hydroxide of high concentration - Google Patents
A kind of preparation method of the exfoliated layered double-hydroxide of high concentration Download PDFInfo
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- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/36—Methods for preparing oxides or hydroxides in general by precipitation reactions in aqueous solutions
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Abstract
The invention discloses a kind of preparation method of the exfoliated layered double-hydroxide of high concentration.Co-precipitation stage, Nano-meter SiO_22Layered double-hydroxide crystal nucleation templates are used as with neopelex；Hydro-thermal stage, layered double-hydroxide rapid growth of crystal, Nano-meter SiO_22Fast transition turns into SiO3 2‑, layered double-hydroxide interlayer is entered by the entrainment of DBSA root anion, SiO is obtained3 2‑/ DBSA root layered double-hydroxide.By the layered double-hydroxide, ultrasonic disperse obtains the exfoliated layered double-hydroxide of highly concentrated nano level in absolute ethyl alcohol.The exfoliated layered double-hydroxide of high concentration made from the inventive method is peeled off at concentrations up to 2g/L in absolute ethyl alcohol through ultrasound.And the present invention has the characteristics of environmental pollution is small, with low cost, yield is higher, it is easy to popularization and application.
Description
Technical field
The invention belongs to technical field of inorganic nonmetallic materials, the double hydroxides of more particularly to a kind of exfoliated stratiform of high concentration
The preparation method of thing.
Background technology
Layered double-hydroxide, is the general designation of an anionoid clay mineral.In its structure, due to isomorphous replacement
Make the positive charge of its main layer board band part, interlayer object contains the anion of exchange, such as carbanion.With the double hydrogen of stratiform
Oxide is the anionic clay minerals of representative with its rigid lamellar structure, high-specific surface area, unique interlamination region environment and layer
Between the characteristic such as controllable modification, be always the focus that clay research worker pays high attention to.Layered double-hydroxide passes through stripping
From the nanoscale twins that acquisition nano flake is positively charged, and other stratified materials stripping product nano lamella is typically negatively charged, this
So that the stripping of layered double-hydroxide has in catalysis, absorption and the multiple fields such as fire-retardant is more widely applied prospect.
Because layered double-hydroxide laminate carries highdensity positive charge, with interlayer anion there is stronger electrostatic to make
Firmly, thus peel off there is certain difficulty.At present, lot of documents report shows the double hydroxides of different guest molecule intercalation stratiforms
Thing, in different decentralized media, peels off concentration also difference.Have been reported (Nie Hongqian etc., Acta PhySico-Chimica Sinica, 2011)
Point out that layered double-hydroxide can realize stripping in short chain alcohol, formamide, but stripping process is complicated, and concentration is undesirable, greatly
Mostly it is partially stripped product.Adachi-Pagano (Adachi-Pagano, M.et al., 2000) is in Chemical
Communications periodicals report the Zn2Al-Cl-LDHs for pointing out Surfactant SDS (SDS) intercalation
Concentration is peeled off up to 1.5g/L through backflow in butanol；Although formamide can effectively realize the double hydrogen of higher concentration (3g/L) stratiform
The stripping (Hibino, T.et al., 2001) of oxide, but be due to that formamide is a kind of noxious material, have unfavorable to environment
Influence, thus its application be subject to certain restrictions.
In recent years, it is whether double from control stratiform in order to seek the more efficient method for preparing nano layered double hydroxides
The nucleating growth process of hydroxide obtains nano layered double hydroxides, or prepares the double hydroxides of stratiform by stripping means
Thing nano flake, has carried out substantial amounts of work.Such as, Chinese patent《A kind of one-step synthesis method peels off hydrotalcite/class neatly
The method of stone》(application publication number：CN103553105A), it is mechanical in dioxygen water environment using soluble metallic salt and urea
The methods such as stirring condensing reflux obtain exfoliated hydrotalcite/houghite.Chinese patent《A kind of simple hydrotalcite stripping side
Method》(Authorization Notice No.：CN101913569B) employ using hydrogen peroxide as reactant, use soluble metallic salt, the thing of alkalescence
Matter, hydrotalcite nano piece has been prepared using hydro-thermal method.Although inventing described method above obtains nanoscale neatly
Stone, but the use of hydrogen peroxide is raw material in methods described, because hydrogen peroxide has a strong oxidizing property and corrosion property, and cost compared with
Height, simultaneous reactions temperature is higher, and energy consumption is big, and synthetic product nanoscale structures difference is big, is not easy to promote.Chinese patent
《A kind of preparation method of exfoliated hydrotalcite》(application publication number：CN103482578A), stratiform pair is made in hydrotalcite calcination
Hydroxy composite metal oxide, is added it in acylate solution, through precipitation separation, washing, vacuum drying, microwave technology
Heating, the hydrotalcite product peeled off.The method and step that the Invention Announce prepares the nano level hydrotalcite peeled off is cumbersome, mistake
Journey is complicated, and manufacturing cycle is longer, is unfavorable for practical application.In summary, the double hydroxides of the compound stratiform of synthesis interlayer anion
Thing, finds a kind of preparation method simple to operate, high-efficiency environment friendly for obtaining layered double-hydroxide ultrathin nanometer lamella, with non-
Often important meaning.
The content of the invention
The invention aims to overcome prior art obtain stripped laminar double-hydroxide technical matters process it is cumbersome,
The shortcomings of low yield, part material have latency environment harm uses coprecipitation with SiO there is provided one kind2And detergent alkylate
Sodium sulfonate is that template supplies layered double-hydroxide crystal nucleation, and layer is obtained for layered double-hydroxide crystal growth by hydro-thermal method
Between anion be SiO3 2-With the layered double-hydroxide of DBSA root, the layered double-hydroxide is placed in anhydrous
The method that ultrasound obtains the ultra-thin lamella of layered double-hydroxide in ethanol.The main advantage of this method is：By the double hydrogen-oxygens of stratiform
Two processes of compound crystal nucleation and growth are independently opened, Nano-meter SiO_22Template is sacrificed as oneself with neopelex,
Nano-meter SiO_2 under hydrothermal condition2Fast transition turns into SiO3 2-, layered double-hydroxide is entered by the entrainment of DBSA root
Interlayer, silicate ion forms steric hindrance between being distributed in alkyl chain, hinders alkyl chain entanglement, alkyl chain can effectively with
Absolute ethyl alcohol is had an effect and deviates from interlamination region, so that layered double-hydroxide main layer board is scattered, obtains the stripping of high concentration
Release ultra-thin lamella (~3nm).Finally conversion enters stratiform pair to the template that the layered double-hydroxide that the present invention is announced is used
Hydroxide interlayer, has broken the conventional technique for needing special step to go template, while the layered double-hydroxide has well
Dispersive property, act on and peeling off without harsh external force, the double hydrogen-oxygens of exfoliated stratiform can be obtained through ultrasound in absolute ethyl alcohol
Compound.
The thinking of the inventive method：By being co-precipitated during offer layered double-hydroxide crystal nucleation, dodecyl
Benzene sulfonic acid sodium salt and SiO2As sacrifice template certainly, and layered double-hydroxide crystal constantly grows under the conditions of hydro-thermal method, SiO2With
Alkali fast reaction generates SiO3 2-, by template from sacrificial action, the double hydroxides of stratiform are entered by the entrainment of DBSA root
Between nitride layer, interlayer anion is obtained for SiO3 2-With the layered double-hydroxide of DBSA root.
Concretely comprise the following steps：
(1) neopelex is added to de- CO20.1~0.2mol/L mixing is configured in deionized water
Liquid, according still further to Nano-meter SiO_22It is 1~2 with neopelex mol ratio:1 measures Nano-meter SiO_22Add above-mentioned mixed liquor
In, it is sufficiently stirred for being formed from template is sacrificed at 60 DEG C, is used as coprecipitation reaction bottom liquid.
(2) using de- CO2Deionized water prepares the NaOH aqueous solution that molar concentration is 1mol/L, as aqueous slkali, simultaneously
Metal ion mol ratio according to divalent metal salt and trivalent metal salt is 3~5:1 is configured to mixed salt solution, 60~
70 DEG C and pH value are that under conditions of 9~10, the aqueous slkali and mixed salt solution of above-mentioned preparation are added with double titration modes
Co-precipitation forms hybrid system in the obtained reaction bottom liquid of step (1), under nitrogen protection atmosphere, is sufficiently stirred for, until above-mentioned
Titration process terminates.
(3) reactant for titrating step (2) after terminating is moved rapidly into reactor, is aged under the conditions of 130~150 DEG C
12~24h, alkyl chain and Nano-meter SiO_22As from template participation layered double-hydroxide growth response is sacrificed, into its interlayer
Domain, is aged through centrifuge washing after terminating, dries, and grinding crosses 200 mesh standard sieves and obtains SiO3 2-/ DBSA root stratiform
Double-hydroxide.
(4) by SiO made from step (3)3 2-/ DBSA root layered double-hydroxide is placed in absolute ethyl alcohol,
Ultrasonic disperse >=4h, that is, be made the exfoliated layered double-hydroxide of high concentration of ultra-thin sheet.
The divalent metal salt is soluble M g2+Salt and solubility Zn2+One kind in salt, trivalent metal salt is solubility
Al3+Salt, solubility Co3+Salt and Dissolvable Fe3+One kind in salt.
The exfoliated layered double-hydroxide of high concentration made from the inventive method peels off concentration in absolute ethyl alcohol through ultrasound
Up to 2g/L.And the present invention has the characteristics of environmental pollution is small, with low cost, yield is higher, it is easy to popularization and application.
Brief description of the drawings
Fig. 1 is layered double-hydroxide (SiO made from the embodiment of the present invention 12- SDBS-LDH) ultra-thin lamella is in anhydrous second
In alcohol it is sonicated after transmission electron micrograph.Layered double-hydroxide lamella is in nanometer thin as we can see from the figure
Piece (as shown by arrows), mutually scatter between piece and piece, its lamellar spacing about 3nm.
Fig. 2 is DBSA root layered double-hydroxide (SDBS-LDH) made from comparative example 1 of the present invention in nothing
In water-ethanol it is sonicated after transmission electron micrograph.Double hydrogen-oxygens of typical large stretch of shape layer by layer as we can see from the figure
Together, dispersiveness is very poor for compound build stack.
Embodiment
The present invention is will be further illustrated in the following examples, but the present invention is not limited.Wherein embodiment 1~3 be
Layered double-hydroxide (the SiO with ultrathin nanometer lamella prepared under the conditions of different parameters2- SDBS-LDH), comparative example 1 is
It is only DBSA root to prepare pure organic layer double-hydroxide (SDBS-LDH), i.e. interlayer ion using same method
Layered double-hydroxide, be used as in absolute ethyl alcohol disperse contrast experiment.
Embodiment 1：
(a) 5.23g neopelexes are added to 100mL and take off CO2It is configured to 0.15mol/L's in deionized water
Mixed liquor, weighs 0.6g Nano-meter SiO_2s2Add in mixed liquor, in the three-necked flask for moving into 500mL, shape is sufficiently stirred at 60 DEG C
Into from template is sacrificed, coprecipitation reaction bottom liquid is used as.
(b) 7.69g (0.03mol) Mg (NO are weighed respectively3)2·6H2O and 3.75g (0.01mol) Al (NO3)3·9H2O,
100mL is dissolved in after mixing and takes off CO2Mixed salt solution is configured in deionized water, 4g NaOH are dissolved in into 100mL takes off CO2
1mol/L aqueous slkali is configured in deionized water, is 65 DEG C in temperature, pH value is controlled in the range of 9.8 ± 0.2, nitrogen protection
Under atmosphere, mixed salt solution and aqueous slkali are added in the obtained reaction bottom liquid of step (a) with double titration modes, fully stirred
Mix, until titration terminates.
(c) reactant for titrating the step of completing (b) is moved rapidly into hydrothermal reaction kettle, be aged under the conditions of 140 DEG C
12h, alkyl chain and Nano-meter SiO_22It is old into its interlamination region as from template participation layered double-hydroxide growth response is sacrificed
Sample centrifuge by change after terminating under 4000rpm centrifugal rotational speeds, through centrifuge washing 5 times after 80 DEG C of dryings, grinding, 200 mesh of mistake
Standard screen obtains SiO3 2-Compound layered double-hydroxide (the SiO of/DBSA root2-SDBS-LDH)。
(d) compound layered double-hydroxide made from 0.1g steps (c) is taken to be placed in 50mL absolute ethyl alcohols, ultrasonic disperse
4h, that is, be made the exfoliated layered double-hydroxide of high concentration, be ultra-thin sheet.
The dispersion that layered double-hydroxide is formed in absolute ethyl alcohol is penetrated using light beam, can be from the vertical of incident light
Tyndall phenomenon is observed in direction, illustrates SiO2- SDBS-LDH dispersion effects in absolute ethyl alcohol are good.Through transmission electron microscope
Analysis, it can be seen that layered double-hydroxide lamella is in nano flake (as shown in the arrow of accompanying drawing 1), mutually disperses between piece and piece
Open, form the exfoliated lamella of high dispersive, its thickness about 3nm.
Embodiment 2：
(a) 6.97g neopelexes are added to 100mL and take off CO2It is configured to 0.20mol/L's in deionized water
Mixed liquor, weighs 0.9g Nano-meter SiO_2s2Add in mixed liquor, in the three-necked flask for moving into 500mL, shape is sufficiently stirred at 60 DEG C
Into from template is sacrificed, coprecipitation reaction bottom liquid is used as.
(b) 7.69g (0.03mol) Mg (NO are weighed respectively3)2·6H2O and 3.75g (0.01mol) Al (NO3)3·9H2O,
100mL is dissolved in after mixing and takes off CO2Mixed salt solution is configured in deionized water, 4g NaOH are dissolved in into 100mL takes off CO2
1mol/L aqueous slkali is configured in deionized water, is 70 DEG C in temperature, pH value control is in 9.5 ± 0.2 scopes, nitrogen protection gas
Under atmosphere, mixed salt solution and aqueous slkali are added in the obtained reaction bottom liquid of step (a) with double titration modes, fully stirred
Mix, until titration terminates.
(c) reactant for titrating the step of completing (b) is moved rapidly into hydrothermal reaction kettle, be aged under the conditions of 140 DEG C
12h, alkyl chain and Nano-meter SiO_22It is old into its interlamination region as from template participation layered double-hydroxide growth response is sacrificed
Sample centrifuge by change after terminating under 4000rpm centrifugal rotational speeds, through centrifuge washing 5 times after 80 DEG C of dryings, grinding, 200 mesh of mistake
Standard screen obtains SiO3 2-The compound layered double-hydroxide of/DBSA root.
(d) compound layered double-hydroxide made from 0.1g steps (c) is taken to be placed in 50mL absolute ethyl alcohols, ultrasonic disperse
4h, that is, be made the exfoliated layered double-hydroxide of high concentration, be ultra-thin sheet.
The dispersion that layered double-hydroxide is formed in absolute ethyl alcohol is penetrated using light beam, can be from the vertical of incident light
Tyndall phenomenon is observed in direction, illustrates that sample dispersion effect in absolute ethyl alcohol is good.Through tem study, energy
It is in nano flake enough to see layered double-hydroxide lamella, and lamellar spacing about 8nm, piece piece is well dispersed, forms exfoliated lamella,
Its lamellar spacing, the diameter of lamella is big compared with embodiment 1.
Embodiment 3：
(a) 5.23g neopelexes are added to 100mL and take off CO2It is configured to 0.15mol/L's in deionized water
Mixed liquor, weighs 0.6g Nano-meter SiO_2s2Add in mixed liquor, in the three-necked flask for moving into 500mL, shape is sufficiently stirred at 60 DEG C
Into from template is sacrificed, coprecipitation reaction bottom liquid is used as.
(b) 8.92g (0.03mol) Zn (NO are weighed respectively3)2·6H2O and 3.75g (0.01mol) Al (NO3)3·9H2O,
100mL is dissolved in after mixing and takes off CO2Mixed salt solution is configured in deionized water, 4g NaOH are dissolved in into 100mL takes off CO2
1mol/L aqueous slkali is configured in deionized water, is 65 DEG C in temperature, pH value control is in 9.8 ± 0.2 scopes, nitrogen protection gas
Under atmosphere, mixed salt solution and aqueous slkali are added in the obtained reaction bottom liquid of step (a) with double titration modes, fully stirred
Mix, until titration terminates.
(c) reactant for titrating the step of completing (b) is moved rapidly into hydrothermal reaction kettle, under 140 DEG C of temperature conditionss
It is aged 12h, alkyl chain and Nano-meter SiO_22As from template participation layered double-hydroxide growth response is sacrificed, into its interlayer
Sample centrifuge by domain, ageing after terminating under 4000rpm centrifugal rotational speeds, through centrifuge washing 5 times after 80 DEG C of dryings, is ground, mistake
200 mesh standard sieves obtain SiO3 2-Compound layered double-hydroxide (the SiO of/DBSA root2-SDBS-LDH)。
(d) compound layered double-hydroxide made from 0.1g steps (c) is taken to be placed in 50mL absolute ethyl alcohols, ultrasonic disperse
4h, that is, be made the exfoliated layered double-hydroxide of high concentration, be ultra-thin sheet.
The dispersion that layered double-hydroxide is formed in absolute ethyl alcohol is penetrated using light beam, can be from the vertical of incident light
Tyndall phenomenon is observed in direction, illustrates that sample dispersion effect in absolute ethyl alcohol is good, but light beam has certain disperse, is disperseed
Effect is poor compared with Examples 1 and 2.Through tem study, it can be seen that layered double-hydroxide lamella is in nano flake,
Piece piece is well dispersed, forms exfoliated lamella, the limellar stripping uniformity is not good enough, there is a little big lamella.
Comparative example 1
(a) 5.23g neopelexes are added to 100mL and take off CO2It is configured to 0.15mol/L's in deionized water
In solution, the three-necked flask for moving into 500mL, it is sufficiently stirred for forming organic formwork at 60 DEG C, is used as the bottom liquid of coprecipitation reaction.
(b) 7.69g (0.03mol) Mg (NO are weighed respectively3)2·6H2O and 3.75g (0.01mol) Al (NO3)3·9H2O,
100mL is dissolved in after mixing and takes off CO2Mixed salt solution is configured in deionized water, 4g NaOH are dissolved in into 100mL takes off CO2
1mol/L aqueous slkali is configured in deionized water.Mixed salt solution and aqueous slkali are added with double titration coprecipitations and walked
Suddenly it is 65 DEG C in temperature, pH value is controlled under 9.8 ± 0.2 scopes, nitrogen protection atmosphere, fully in (a) obtained reaction bottom liquid
Until titration terminates under stirring condition.
(c) reactant for titrating the step of completing (b) is moved rapidly into hydrothermal reaction kettle, under 140 DEG C of temperature conditionss
It is aged 12h, alkyl chain and Nano-meter SiO_22As from template participation layered double-hydroxide growth response is sacrificed, into its interlayer
Domain, ageing centrifuges sample by sample after terminating under 4000rpm centrifugal rotational speeds, through centrifuge washing 5 times after 80 DEG C of dryings,
Grinding, crosses 200 mesh standard sieves and obtains the layered double-hydroxide (SDBS-LDH) that interlayer anion is DBSA root.
(d) layered double-hydroxide made from 0.1g steps (c) is taken to be placed in 50mL absolute ethyl alcohols, ultrasonic disperse 4h is obtained
Obtain organic layer double-hydroxide and disperse comparative sample.
The dispersion that SDBS-LDH is formed in absolute ethyl alcohol is penetrated using light beam, observed from the vertical direction of incident light
Light path passes through dispersion light beam disperse, it is impossible to form bright " light path ", illustrate SDBS-LDH in absolute ethyl alcohol dispersion effect compared with
Difference, peeling effect is undesirable.Through tem study, it can be seen that typical sheet layer layered double-hydroxide structure
It is stacked, dispersiveness is very poor, it is impossible to obtain the exfoliated laminated double hydroxide nanometer lamella of high dispersive.
Claims (1)
1. a kind of preparation method of the exfoliated layered double-hydroxide of high concentration, it is characterised in that concretely comprise the following steps：
(1) neopelex is added to de- CO20.1 ~ 0.2 mol/L mixed liquor is configured in deionized water, then
According to Nano-meter SiO_22It is 1 ~ 2 with neopelex mol ratio:1 measures Nano-meter SiO_22Add in above-mentioned mixed liquor, 60
It is sufficiently stirred for being formed from template is sacrificed at DEG C, is used as coprecipitation reaction bottom liquid；
(2) using de- CO2Deionized water prepares the NaOH aqueous solution that molar concentration is 1 mol/L, as aqueous slkali, while according to
The metal ion mol ratio of divalent metal salt and trivalent metal salt is 3 ~ 5:1 is configured to mixed salt solution, at 60 ~ 70 DEG C and
PH value be 9 ~ 10 under conditions of, by the aqueous slkali and mixed salt solution of above-mentioned preparation with double titration modes add step (1)
Co-precipitation forms hybrid system in the liquid of obtained reaction bottom, under nitrogen protection atmosphere, is sufficiently stirred for, until above-mentioned titration process
Terminate；
(3) by step (2) titrate terminate after reactant be moved rapidly into reactor, under the conditions of 130 ~ 150 DEG C be aged 12 ~
24h, alkyl chain and Nano-meter SiO_22It is old into its interlamination region as from template participation layered double-hydroxide growth response is sacrificed
Change through centrifuge washing after terminating, dry, grinding crosses 200 mesh standard sieves and obtains SiO3 2-The double hydrogen of/DBSA root stratiform
Oxide；
(4) by SiO made from step (3)3 2-/ DBSA root layered double-hydroxide is placed in absolute ethyl alcohol, is surpassed
Sound disperses >=4 h, that is, the exfoliated layered double-hydroxide of high concentration of ultra-thin sheet is made；
The divalent metal salt is soluble M g2+Salt and solubility Zn2+One kind in salt, trivalent metal salt is solubility Al3+
Salt, solubility Co3+Salt and Dissolvable Fe3+One kind in salt.
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